Process of making carbon tetrachlorid.



PATENTED JUNE 30, 1908.

G. E. AGKER.

PROCESS OF MAKING CARBON TETRAGHLORID.

APPLICATION FILED JULY 19, 1904. RENEWED D30. 4, 1907.

RVGJZIOT chlorination of the dissolved sulfur.

UNITED STATES PATENT oFFroE.

CHARLES ERNEST AOKER, OF NIAGARA FALLS, NEIV YORK, ASSIGNOR, BY MESNE ASSIGN- MENTS, TO MARCUS STINE, OF NEW YORK, N. Y.

PROCESS OF MAKING CARBON TETRACHLORID.

Specification of Letters Patent.

Patented June 30,11908.

Applicationfilegl, .luly 18, 1904, Serial No.'217,127 Renewed December 4, 1907. Serial No. 405,097.

To all whom it may'concern: I

' Be it known that I, CHAItiLES EnNEsT Across, a citizen of -theUnited States, residingat Niagara Falls, in the county of Niagara D and State of New York, have invented certain new and useful Improvements in Processes of Making Carbon Tetrachlorid,- of which the following is a s ecification.

In an application Seria Number 217,126, filed July18th, 1904, I have described and claimed a process of pro'ducingsulfur chlorids by subjecting a solution of sulfur in sulfur chlorid to the action of' a gaseous body containing chlorin, dissolving more'sulfur in the product and'repeating the cycle of operations.

Accordingto the present process, the sulfur chlorid produced by the specifiedmethod is caused to react on carbon disulfid to produce carbon tetrachlorid and sulfur. The sulfur is then redissolved in sulfur chlorid and the cycle is continuously repeated.

-An a p'aratus for carrying out the first stage 0 the process is shown in the accompan ing drawing, in which the figure is a vertical section through the solution tank, storage reservoir and reaction tower.

The tank 1 in which the solution of the sulfur in the sulfur chloridis effected, is preferably an iron vessel with. a lining 2 of lead. The sulfur 3 is introduced through an openings and lies on the bottom of the tank, a transverse dam 5 bein rovided toleave a well 6 for the clear 0 ution. A pipe 7, which may be of hard lead, leads upward from the tank 1 through a pump 8 to the storage reservoir 9. A pipe 10 having a cock delivers the solution into the upper end of the reaction tower 11. This tower is shown as of the Rohrmann type but may be of any preferred construction. The dry chlorin gas,

which may contain air or oxygen but should be of fair strength, is introduced into the lower end of the tower through a assage 12 and the waste gases are withdrawn y suction from the upper end through a passage 13. The tower is provided with interposed coolin sections '14 through which water is circu ated to remove the heat produced by 1the e temperature'of the liquid is preferably maintained at a olpoint varying from normal to or-YO? C. t is, of course, necessary to maintain it below the distillation point of the monochlorid. The liquid is" returned to the 35 solution tank bya pipe 15 le ading from the of liquid is passed through the reaction tower' and 1t is subjected to an excess of chlorin. Chlorin may also be introduced directly into the solution tank. maintain the temperature in the system below the volatilizing 68 0., as by and It is also necessary to point of the dichlorid assmg refrigerated brine through the coo ing sections of the tower and jacketing the solution tank.

In the second stage of the process, a portion of the sulfur chlorid or mixture of chloride is withdrawn from the reaction tower or solution tank and introduced into a diester, which may be of iron lined with lead. faarbon disulfid is also supplied to the digester in amount sufficient to provide one atom of carbon for each four atoms of chlorin in the chlorid or chlorids The liquids in the di ester are then mixed and heated, preferab y to about 60 C., until all of the chlorin in the chlorids has combined with the carbon in the sulfid to produce carbon tetrachlorid. The reactions are indicated by the following formulae:

The carbon tetrachlorid may be distilled off and the sulfur set free b the reaction crystallized out of the res'idua li uid. This sulfur is then returned to the so ution tank and em loyed to producefurther quantities of the sulfur chlorid, the process thus being continuous or cyclical.

I claim 1. In the process of making carbon tetra-a;

chlorid those steps which consist first, in dissolving sulfur in sulfur chlorid; second, subjecting said solution in a finely divided state to the action of a gaseous body containing chlorin, and third, causing the resulting 'flul to react on carbon disulfid. v

2. In the process of making carbon tetrachlorid those steps which consist first, in dissolving sulfur in sulfur chlorid, second, subto the action of a gaseous bod 'jecting said solution in a finely divided state tothe action of a gaseous body containing chlorin, third, causin the resulting fluid to react on carbon disu d and fourth, dissolvin the sulfur freed by the reaction in sulfur c orid.

3. In the process of making carbon tetrachlorid those steps which consist first, in dissolving sulfur in sulfur chlorid, second, sub- 1' ecting said solution in a finely divided state containing chlorin, third, causin the resu ting fluid to react on carbon disu d, and fourth distilling off the carbon tetrachlorid.

4. In the process of making carbon tetrachlorid'those' steps which consist first in dissolving sulfur in sulfur chlorid, second, subjecting said solution in a finely divided state to'the action of a gaseous body ,containing chlorin, third, causin the resulting fluid to react on carbon disu d, fourth, distilling 05 the carbon tetrachlorid, and fifth, dissolving the residual sulfur in sulfur chlorid.

5. In the process of making carbon tetrachlorid those steps which consist first in dissolving sulfur in sulfur chlorid, second, subjecting said solution in a finely divided state to the action of a gaseous body containing chlorin, third, causin the resulting fluid to react on carbon disul d, fourth, distilling off the carbon tetrachlorid, and fifth, dissolving the residual sulfur in sulfur chlorid and repeating the cycle of o erations.

6. In the process 0 making carbon tetrachlorid those steps which consist first in dissolving sulfur in sulfur chlorid, second, subjecting said solution in a finely divided state to the action of a gaseous body containing chlorin and a diluent, and third causin the resulting fluid to react on carbon disulfid.

In testimony whereof, I affix my signature in presence of two witnesses.

CHARLES ERNEST ACKER.

Witnesses:

GERALDINE M. MCBRIDE, JOSEPHINE F. KE UG 

